JP2000329714A - X-ray fluorescence analyzer - Google Patents
X-ray fluorescence analyzerInfo
- Publication number
- JP2000329714A JP2000329714A JP11142743A JP14274399A JP2000329714A JP 2000329714 A JP2000329714 A JP 2000329714A JP 11142743 A JP11142743 A JP 11142743A JP 14274399 A JP14274399 A JP 14274399A JP 2000329714 A JP2000329714 A JP 2000329714A
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- Japan
- Prior art keywords
- fluorescent
- rays
- semiconductor detector
- sample
- ray
- Prior art date
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- Analysing Materials By The Use Of Radiation (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、検出器として半導
体検出器のみを用いた蛍光Ｘ線分析装置に関するもので
ある。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray fluorescence analyzer using only a semiconductor detector as a detector.
【０００２】[0002]
【従来の技術】従来のいわゆる波長分散型の蛍光Ｘ線分
析装置においては、検出器として、例えば、Ａl 程度に
軽い元素の分析用にはガスフロー型比例計数管（Ｆ−Ｐ
Ｃ）を、Ｆe 、Ｓn 等程度に重い元素の分析用にはシン
チレーション計数管（ＳＣ）を用い、各検出器に適した
分光素子等の光学系を組み合わせて分光している。2. Description of the Related Art In a conventional so-called wavelength dispersive X-ray fluorescence spectrometer, a gas flow type proportional counter (FP) is used as a detector, for example, for the analysis of elements as light as Al.
C) is analyzed by using a scintillation counter (SC) for the analysis of elements as heavy as Fe, Sn, etc., using an optical system such as a spectroscopic element suitable for each detector.
【０００３】[0003]
【発明が解決しようとする課題】しかし、このような装
置では、検出器を少なくとも２種類備えねばならないた
め構成が複雑で、しかも、エネルギー分解能が低い等の
検出器の特性から、装置の感度や精度が必ずしも十分で
ないため、今一つ正確な分析ができない。一方、従来の
いわゆるエネルギー分散型の蛍光Ｘ線分析装置では、エ
ネルギー分解能の高い半導体検出器（ＳＳＤ）を用いる
が、検出器に大がかりな冷却装置が必要となることが多
く走査が困難なこともあって分光素子を用いないため、
検出器の分解能で装置の分解能が決まる。ここで、一般
に、蛍光Ｘ線分析装置における分解能は、Ａl やＦe 程
度に軽い元素の分析では、適切な分光素子を用いた波長
分散型が優れ、Ｍo 程度以上に重い元素の分析では、半
導体検出器を用いたエネルギー分散型が優れる。したが
って、従来のエネルギー分散型の蛍光Ｘ線分析装置にお
いては、Ａl やＦe 程度に軽い元素の分析では、装置の
精度が必ずしも十分でなく、やはり今一つ正確な分析が
できない。However, in such an apparatus, since at least two types of detectors must be provided, the structure is complicated, and the sensitivity of the apparatus is low due to the characteristics of the detector such as low energy resolution. Since the accuracy is not always sufficient, accurate analysis cannot be performed. On the other hand, a conventional so-called energy dispersive X-ray fluorescence spectrometer uses a semiconductor detector (SSD) having a high energy resolution. However, a large-scale cooling device is required for the detector, which makes scanning difficult. Because there is no spectral element
The resolution of the device is determined by the resolution of the detector. Here, in general, the resolution of a fluorescent X-ray analyzer is excellent in the wavelength dispersion type using an appropriate spectroscopic element in the analysis of elements as light as Al or Fe, and in semiconductor analysis in the analysis of elements heavier than Mo or more. Energy dispersing type using a vessel is excellent. Therefore, in the conventional energy dispersive X-ray fluorescence spectrometer, the accuracy of the device is not always sufficient for the analysis of an element as light as Al or Fe, so that another accurate analysis cannot be performed.
【０００４】本発明は前記従来の問題に鑑みてなされた
もので、検出器として半導体検出器のみを用いた簡単な
構成で、精度や感度が高く十分正確な分析ができる蛍光
Ｘ線分析装置を提供することを目的とする。SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned conventional problems, and provides a fluorescent X-ray analyzer which has a simple configuration using only a semiconductor detector as a detector and has high accuracy and sensitivity and can perform sufficiently accurate analysis. The purpose is to provide.
【０００５】[0005]
【課題を解決するための手段】前記目的を達成するため
に、請求項１の蛍光Ｘ線分析装置は、まず、試料が載置
される試料台と、試料に１次Ｘ線を照射するＸ線源と、
試料から発生した蛍光Ｘ線を通過させるスリットとを備
えている。また、分光素子を複数種類有し、前記スリッ
トを通過する蛍光Ｘ線の光路に選択的に進出させて入射
した蛍光Ｘ線を分光させる分光素子交換器と、前記分光
素子で分光された蛍光Ｘ線の強度を測定する半導体検出
器とを備えている。さらに、前記分光素子で分光される
蛍光Ｘ線の波長を変えながら、その分光された蛍光Ｘ線
が前記半導体検出器に入射するように、前記スリット、
分光素子交換器および半導体検出器のうち少なくとも分
光素子交換器および半導体検出器を連動させる連動手段
を備えている。In order to achieve the above object, an X-ray fluorescence spectrometer according to a first aspect of the present invention comprises a sample stage on which a sample is placed and an X-ray for irradiating the sample with primary X-rays. Source,
And a slit for passing fluorescent X-rays generated from the sample. A spectroscopic element exchanger that has a plurality of types of spectroscopic elements and selectively advances to an optical path of the fluorescent X-rays passing through the slit to split the incident fluorescent X-rays; A semiconductor detector for measuring the intensity of the line. Further, while changing the wavelength of the fluorescent X-rays split by the spectroscopic element, the slit, so that the split fluorescent X-rays are incident on the semiconductor detector.
There is provided interlocking means for interlocking at least the spectral element exchanger and the semiconductor detector among the spectral element exchanger and the semiconductor detector.
【０００６】請求項１の装置によれば、まず、検出器と
して半導体検出器のみを用いるので構成が簡単である。
また、かかる連動手段により広い波長範囲の蛍光Ｘ線に
対応しつつ、Ａl やＦe 程度に軽い元素の分析では、適
切な分光素子を選択して用いるので分解能に優れ、Ｍo
程度以上に重い元素の分析では、半導体検出器を用いて
いるのでやはり分解能に優れる。したがって、精度が高
く十分正確な分析ができる。According to the first aspect of the present invention, first, only the semiconductor detector is used as the detector, so that the configuration is simple.
In addition, in the analysis of an element as light as Al or Fe while selecting an appropriate spectroscopic element and using it, it is excellent in resolution and Mo, while responding to fluorescent X-rays in a wide wavelength range by such interlocking means.
In the analysis of an element that is heavier than that, a semiconductor detector is used, so that the resolution is also excellent. Therefore, highly accurate and sufficiently accurate analysis can be performed.
【０００７】請求項２の蛍光Ｘ線分析装置は、請求項１
の装置において、前記半導体検出器を、試料から発生し
た蛍光Ｘ線の強度を前記スリットおよび分光素子を介さ
ずに測定する位置に移動させる移動手段を備える。[0007] The fluorescent X-ray analyzer according to the second aspect is the first aspect.
In the apparatus, a moving means for moving the semiconductor detector to a position where the intensity of the fluorescent X-ray generated from the sample is measured without passing through the slit and the spectral element.
【０００８】請求項２の装置によれば、かかる移動手段
により、試料から発生した蛍光Ｘ線をスリットや分光素
子を介さずに直接半導体検出器に入射できるので、試料
の微小部位を分析する場合等、蛍光Ｘ線の強度が微弱な
場合でも高いＳ／Ｎ比で測定できる。したがって、感度
が高く十分正確な分析ができる。According to the second aspect of the present invention, the X-rays generated from the sample can be directly incident on the semiconductor detector without passing through a slit or a spectroscopic element by the moving means. For example, even when the intensity of the fluorescent X-ray is weak, it can be measured at a high S / N ratio. Therefore, highly sensitive and sufficiently accurate analysis can be performed.
【０００９】請求項３の蛍光Ｘ線分析装置は、まず、試
料が載置される試料台と、試料に１次Ｘ線を照射するＸ
線源と、試料から発生した蛍光Ｘ線を通過させるスリッ
トとを備えている。また、そのスリットを通過した蛍光
Ｘ線の一部を反射する全反射ミラーと、その全反射ミラ
ーで反射された蛍光Ｘ線の強度を測定する半導体検出器
とを備えている。さらに、前記全反射ミラーで反射され
る蛍光Ｘ線の波長帯域を変え、その反射された蛍光Ｘ線
が前記半導体検出器に入射するように、前記スリット、
全反射ミラーおよび半導体検出器のうち少なくとも全反
射ミラーを回動させる回動手段を備えている。According to a third aspect of the present invention, there is provided an X-ray fluorescence spectrometer comprising: a sample stage on which a sample is placed;
It has a radiation source and a slit for passing fluorescent X-rays generated from the sample. In addition, a total reflection mirror that reflects a part of the fluorescent X-rays passing through the slit, and a semiconductor detector that measures the intensity of the fluorescent X-rays reflected by the total reflection mirror are provided. Further, changing the wavelength band of the fluorescent X-rays reflected by the total reflection mirror, the slit, so that the reflected fluorescent X-rays are incident on the semiconductor detector.
A rotation means for rotating at least the total reflection mirror among the total reflection mirror and the semiconductor detector is provided.
【００１０】請求項３の装置によれば、まず、検出器と
して半導体検出器のみを用いるので構成が簡単である。
また、かかる回動手段により広い波長範囲の蛍光Ｘ線に
対応しつつ、Ａl やＦe 程度に軽い元素の分析では、全
反射ミラーで所望の波長帯域の蛍光Ｘ線のみを反射させ
るので分解能に優れ、Ｍo 程度以上に重い元素の分析で
は、半導体検出器を用いているのでやはり分解能に優れ
る。さらに、分光素子に比べはるかに反射効率の高い全
反射ミラーを用いるので、装置としてもＳ／Ｎ比が高
い。したがって、精度や感度が高く十分正確な分析がで
きる。According to the third aspect of the present invention, the configuration is simple because only the semiconductor detector is used as the detector.
In addition, in the analysis of elements as light as Al and Fe while reflecting the fluorescent X-rays in a wide wavelength range by such a rotating means, the total reflection mirror reflects only the fluorescent X-rays in a desired wavelength band, so that the resolution is excellent. In the analysis of elements heavier than Mo or higher, the resolution is also excellent because a semiconductor detector is used. Further, since a total reflection mirror having a much higher reflection efficiency than that of the spectral element is used, the S / N ratio is high as an apparatus. Therefore, highly accurate and sensitive analysis can be performed with sufficient accuracy.
【００１１】[0011]
【発明の実施の形態】以下、本発明の第１実施形態の装
置について説明する。まず、この装置の構成について、
図１にしたがって説明する。この装置は、試料１が載置
される試料台２と、試料１に１次Ｘ線３を照射するＸ線
管等のＸ線源４と、試料１から発生した蛍光Ｘ線５を通
過させるソーラスリット１１とを備えている。また、分
光素子６を例えば２種類有し、ソーラスリット１１を通
過する蛍光Ｘ線１３の光路に選択的に進出させて入射し
た蛍光Ｘ線１３を分光させる分光素子交換器１４と、分
光素子６で分光された蛍光Ｘ線７の強度を測定する半導
体検出器８とを備えている。さらに、分光素子６で分光
される蛍光Ｘ線７の波長を変えながら、その分光された
蛍光Ｘ線７が半導体検出器８に入射するように、分光素
子交換器１４および半導体検出器８を連動させる連動手
段１０を備えている。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An apparatus according to a first embodiment of the present invention will be described below. First, regarding the configuration of this device,
This will be described with reference to FIG. This apparatus allows a sample table 2 on which a sample 1 is mounted, an X-ray source 4 such as an X-ray tube for irradiating the sample 1 with primary X-rays 3, and a fluorescent X-ray 5 generated from the sample 1 to pass therethrough. And a solar slit 11. Further, a spectroscopic element exchanger 14 having, for example, two types of spectroscopic elements 6, which selectively advances to the optical path of the fluorescent X-rays 13 passing through the solar slit 11 and splits the incident fluorescent X-rays 13, And a semiconductor detector 8 for measuring the intensity of the fluorescent X-rays 7 that have been spectrally separated. Further, while changing the wavelength of the fluorescent X-rays 7 separated by the spectral element 6, the spectroscopic element exchanger 14 and the semiconductor detector 8 are linked so that the separated fluorescent X-rays 7 enter the semiconductor detector 8. There is provided an interlocking means 10 for causing the operation.
【００１２】ここで、２種類の分光素子６Ａ，６Ｂは、
例えば、Pentaerythritol （ＰＥＴ）とＬi Ｆである。
半導体検出器８としては、シリコン検出器（Ｓi(Ｌ
i)）、ゲルマニウム検出器、シリコンドリフト検出器
（ＳＤＤ）、超伝導放射線検出器（ＳＴＪ）等の固体素
子を用いることができる。特に、液体窒素によらずPert
ier素子による冷却を行うものが、コンパクトで本発明
の実施に適している。Here, the two types of spectral elements 6A and 6B are:
For example, Pentaerythritol (PET) and LiF.
As the semiconductor detector 8, a silicon detector (Si (L
i)), a solid-state device such as a germanium detector, a silicon drift detector (SDD), and a superconducting radiation detector (STJ) can be used. In particular, Pert regardless of liquid nitrogen
The one that performs cooling by an ier element is compact and suitable for implementing the present invention.
【００１３】連動手段１０は、いわゆるゴニオメータで
ある。蛍光Ｘ線１３がある入射角θで分光素子６Ａへ入
射すると、その蛍光Ｘ線１３の延長線９と分光素子６Ａ
で分光（回折）された蛍光Ｘ線７は入射角θの２倍の分
光角２θをなすが、連動手段１０は、分光角２θを変え
て分光される蛍光Ｘ線７の波長を変えながら、その分光
された蛍光Ｘ線７が半導体検出器８に入射するように、
分光素子６Ａを、分光素子交換器１４を介して、分光素
子６Ａの表面の中心を通る紙面に垂直な軸Ｏを中心に回
転させ、その回転角の２倍だけ、半導体検出器８を、軸
Ｏを中心に円１２に沿って回転（走査）させる。連動手
段１０において、例えば、前記軸Ｏに取り付けたポテン
ショメータ等により、分光素子６Ａおよび半導体検出器
８が回転した結果形成される入射角θ、分光角２θが確
認される。The interlocking means 10 is a so-called goniometer. When the fluorescent X-rays 13 enter the spectroscopic element 6A at a certain incident angle θ, the extension line 9 of the fluorescent X-rays 13 and the spectroscopic element 6A
The fluorescent X-rays 7 spectrally (diffracted) at 2 form a spectral angle 2θ twice the incident angle θ, but the interlocking means 10 changes the spectral angle 2θ to change the wavelength of the fluorescent X-rays 7 In order that the separated fluorescent X-rays 7 enter the semiconductor detector 8,
The spectroscopic element 6A is rotated via the spectroscopic element exchanger 14 about an axis O perpendicular to the paper surface passing through the center of the surface of the spectroscopic element 6A, and the semiconductor detector 8 is rotated by twice the rotation angle. It is rotated (scanned) along the circle 12 around O. In the interlocking means 10, the incident angle θ and the spectral angle 2θ formed as a result of rotation of the spectroscopic element 6A and the semiconductor detector 8 are confirmed by, for example, a potentiometer attached to the axis O.
【００１４】なお、連動手段１０は、分光素子交換器１
４と半導体検出器８を歯車機構等の駆動機構により機械
的に連結し、その歯車機構等を単一のモータ等の駆動源
で駆動するものでもよいし、分光素子交換器１４と半導
体検出器８をそれぞれ独立した駆動源および駆動機構で
駆動し、それらの駆動源を適切に制御して前記のような
動作を実現するものでもよい。The interlocking means 10 is connected to the spectral element exchanger 1
4 and the semiconductor detector 8 may be mechanically connected by a drive mechanism such as a gear mechanism, and the gear mechanism or the like may be driven by a single drive source such as a motor, or the spectral element exchanger 14 and the semiconductor detector 8 may be driven by independent drive sources and drive mechanisms, and the above-described operation may be realized by appropriately controlling the drive sources.
【００１５】さらに、この装置は、図２に示すように、
半導体検出器８を、試料１から発生した蛍光Ｘ線５の強
度をソーラスリット１１および分光素子６を介さずに測
定する位置に移動させる移動手段１５を備える。この移
動にあたり、ソーラスリット１１や分光素子交換器１４
が干渉しないよう退避させる必要があれば、移動手段１
５は、それらを退避させることも行う。なお、移動手段
１５も、モータ等の駆動源および歯車機構等の駆動機構
からなるが、連動手段１０と別個独立のものでもよく、
連動手段１０と少なくとも一部が共通するものでもよ
い。[0015] Further, as shown in FIG.
The semiconductor detector 8 includes a moving unit 15 for moving the intensity of the fluorescent X-rays 5 generated from the sample 1 to a position where the intensity is measured without passing through the solar slit 11 and the spectral element 6. In this movement, the solar slit 11 and the spectral element exchanger 14
If it is necessary to evacuate to avoid interference,
5 also evacuates them. The moving means 15 also includes a driving source such as a motor and a driving mechanism such as a gear mechanism, but may be independent of the interlocking means 10.
At least part of the interlocking means 10 may be common.
【００１６】次に、この装置の動作について説明する。
まず、例えばＡl 程度に軽い元素について分析する場合
には、図１の分光素子交換器１４が紙面に垂直な中心軸
Ｐを中心にして回転され、適切なＰＥＴの分光素子６Ａ
が、ソーラスリット１１を通過する蛍光Ｘ線１３の光路
に進出するように選択される。そして、試料台２に載置
された試料１にＸ線源４から１次Ｘ線３が照射される
と、試料１から発生した蛍光Ｘ線５がソーラスリット１
１を通過し、分光素子６Ａで分光され、分光された蛍光
Ｘ線７の強度が半導体検出器８で測定される。ここで、
分光素子６Ａと半導体検出器８を連動手段１０で連動さ
せることにより、試料１から発生した蛍光Ｘ線５を、ソ
ーラスリット１１を通過させてまず分光素子６Ａでそれ
ぞれの波長に光学的に分光し、さらにエネルギー分解能
の高い半導体検出器８および図示しない波高分析器で電
気的に詳細に分離して検出する。Next, the operation of this device will be described.
First, when analyzing an element as light as Al, for example, the spectroscopic element exchanger 14 of FIG. 1 is rotated about a central axis P perpendicular to the plane of the drawing, and an appropriate PET spectroscopic element 6A is analyzed.
Is selected to enter the optical path of the fluorescent X-ray 13 passing through the solar slit 11. When the primary X-ray 3 is irradiated from the X-ray source 4 to the sample 1 placed on the sample stage 2, the fluorescent X-rays 5 generated from the sample 1
1 and is separated by the spectroscopic element 6A, and the intensity of the separated fluorescent X-ray 7 is measured by the semiconductor detector 8. here,
By interlocking the spectroscopic element 6A and the semiconductor detector 8 with the interlocking means 10, the fluorescent X-rays 5 generated from the sample 1 are passed through the solar slit 11 and first optically split into the respective wavelengths by the spectroscopic element 6A. In addition, the semiconductor detector 8 having a higher energy resolution and a wave height analyzer (not shown) electrically separate and detect the electric power.
【００１７】また、例えばＦe 程度以上に重い元素につ
いて分析する場合には、分光素子交換器１４が紙面に垂
直な中心軸Ｐを中心にして回転され、適切なＬi Ｆの分
光素子６Ｂが、ソーラスリット１１を通過する蛍光Ｘ線
１３の光路に進出するように選択される。以下、前記と
同様に各波長の蛍光Ｘ線５が分光、検出される。In the case of analyzing an element heavier than Fe, for example, the spectroscopic element exchanger 14 is rotated about a central axis P perpendicular to the plane of the drawing, and an appropriate LiF spectroscopic element 6B is It is selected so as to enter the optical path of the fluorescent X-ray 13 passing through the slit 11. Thereafter, the fluorescent X-rays 5 of each wavelength are separated and detected in the same manner as described above.
【００１８】このように、第１実施形態の装置によれ
ば、まず、検出器として半導体検出器８のみを用いるの
で構成が簡単である。また、かかる連動手段１０により
広い波長範囲の蛍光Ｘ線５に対応しつつ、Ａl やＦe 程
度に軽い元素の分析では、適切な分光素子６Ａ，６Ｂを
選択して用いるので分解能に優れ、Ｍo 程度以上に重い
元素の分析では、半導体検出器８を用いているのでやは
り分解能に優れる。したがって、精度が高く十分正確な
分析ができる。なお、Ｆe 程度以上に重い元素のうち、
Ｍo 程度以上に重い元素の分析については、半導体検出
器８および波高分析器による電気的なエネルギー分解の
みで十分で、分光素子６は必要でない。As described above, according to the apparatus of the first embodiment, first, only the semiconductor detector 8 is used as the detector, so that the configuration is simple. In addition, in the analysis of elements as light as Al and Fe while selecting the appropriate spectroscopic elements 6A and 6B while using the interlocking means 10 to cope with the fluorescent X-rays 5 in a wide wavelength range, the resolution is excellent, and about Mo. In the analysis of heavy elements as described above, the semiconductor detector 8 is used, so that the resolution is also excellent. Therefore, highly accurate and sufficiently accurate analysis can be performed. Among the elements heavier than Fe,
For analysis of elements heavier than Mo, only electrical energy decomposition by the semiconductor detector 8 and the pulse height analyzer is sufficient, and the spectroscopic element 6 is not required.
【００１９】続けて、試料１の微小部位を分析する場合
等（試料１全体が微小である場合も含む）、蛍光Ｘ線５
の強度が微弱な場合の動作について説明する。まず、図
２に示すように、移動手段１５により、半導体検出器８
を、試料１から発生した蛍光Ｘ線５の強度をソーラスリ
ット１１および分光素子６を介さずに測定する位置に移
動させ、試料台２に載置された試料１に近接させる。そ
して、試料１にＸ線源４から１次Ｘ線３が照射される
と、試料１から発生した蛍光Ｘ線５が、直接半導体検出
器８に入射して、エネルギー分解能の高い半導体検出器
８および波高分析器で電気的に分離して検出される。こ
のように、第１実施形態の装置によれば、かかる移動手
段１５により、試料１から発生した蛍光Ｘ線５を、ソー
ラスリット１１や分光素子６を介さずに直接半導体検出
器８に入射させることもできるので、試料１から発生す
る蛍光Ｘ線５の強度が微弱な場合でも、高いＳ／Ｎ比で
測定できる。したがって、感度が高く十分正確な分析が
できる。Subsequently, when analyzing a minute portion of the sample 1 (including a case where the whole sample 1 is minute), the fluorescent X-ray 5
The operation in the case where the intensity is weak is described. First, as shown in FIG.
Is moved to a position where the intensity of the fluorescent X-rays 5 generated from the sample 1 is measured without passing through the solar slit 11 and the spectroscopic element 6, and is brought close to the sample 1 placed on the sample stage 2. When the sample 1 is irradiated with the primary X-rays 3 from the X-ray source 4, the fluorescent X-rays 5 generated from the sample 1 are directly incident on the semiconductor detector 8 and have high energy resolution. And electrically separated by a wave height analyzer. Thus, according to the apparatus of the first embodiment, the moving means 15 causes the fluorescent X-rays 5 generated from the sample 1 to directly enter the semiconductor detector 8 without passing through the solar slit 11 or the spectroscopic element 6. Therefore, even when the intensity of the fluorescent X-rays 5 generated from the sample 1 is weak, the measurement can be performed at a high S / N ratio. Therefore, highly sensitive and sufficiently accurate analysis can be performed.
【００２０】次に、本発明の第２実施形態の装置につい
て説明する。まず、この装置の構成について、図３にし
たがって説明する。この装置は、試料１が載置される試
料台２と、試料１に１次Ｘ線３を照射するＸ線管等のＸ
線源４と、試料１から発生した蛍光Ｘ線５を通過させる
ソーラスリット１１とを備えている。また、そのソーラ
スリット１１を通過した蛍光Ｘ線１３の一部を反射する
全反射ミラー１６と、その全反射ミラー１６で反射され
た蛍光Ｘ線１７の強度を測定する半導体検出器８とを備
えている。さらに、全反射ミラー１６で反射される蛍光
Ｘ線１７の波長帯域を変え、その反射された蛍光Ｘ線１
７が半導体検出器８に入射するように、全反射ミラー１
６および半導体検出器８を回動させる回動手段１８を備
えている。ここで、全反射ミラー１６は、例えばソーダ
ライムガラス製で、半導体検出器８は、第１実施形態と
同様のものを用いることができる。Next, an apparatus according to a second embodiment of the present invention will be described. First, the configuration of this device will be described with reference to FIG. The apparatus includes a sample table 2 on which a sample 1 is placed and an X-ray tube or the like for irradiating the sample 1 with primary X-rays 3.
The apparatus includes a radiation source 4 and a solar slit 11 through which fluorescent X-rays 5 generated from the sample 1 pass. Further, a total reflection mirror 16 that reflects a part of the fluorescent X-rays 13 passing through the solar slit 11 and a semiconductor detector 8 that measures the intensity of the fluorescent X-rays 17 reflected by the total reflection mirror 16 are provided. ing. Further, the wavelength band of the fluorescent X-rays 17 reflected by the total reflection mirror 16 is changed, and the reflected fluorescent X-rays 1 are changed.
7 so that the total reflection mirror 1 is incident on the semiconductor detector 8.
6 and a rotation means 18 for rotating the semiconductor detector 8. Here, the total reflection mirror 16 is made of, for example, soda-lime glass, and the same semiconductor detector 8 as that of the first embodiment can be used.
【００２１】全反射ミラー１６は、視斜角φで入射する
蛍光Ｘ線１３のうち、全反射の臨界角がφよりも大きい
蛍光Ｘ線１７を全反射し、それ以外の蛍光Ｘ線を吸収す
る。一般に、エネルギーの低い、すなわち波長の長い蛍
光Ｘ線ほど全反射の臨界角が大きいから、視斜角φを所
望の蛍光Ｘ線１７の臨界角よりもわずかに小さく設定す
れば、所望の蛍光Ｘ線１７よりもエネルギーの高い、す
なわち波長の短い蛍光Ｘ線を全反射ミラー１６に吸収さ
せることにより、不要な励起線３等を除去できる。The total reflection mirror 16 totally reflects the fluorescent X-rays 17 of which the critical angle of total reflection is larger than φ among the fluorescent X-rays 13 incident at the oblique angle φ, and absorbs the other fluorescent X-rays. I do. In general, a fluorescent X-ray having a lower energy, that is, a longer wavelength, has a larger total reflection critical angle. Therefore, if the viewing angle φ is set slightly smaller than the critical angle of the desired fluorescent X-ray 17, the desired fluorescent X-ray can be obtained. By causing the total reflection mirror 16 to absorb fluorescent X-rays having higher energy than the line 17, that is, having a shorter wavelength, unnecessary excitation lines 3 and the like can be removed.
【００２２】回動手段１８は、このように全反射ミラー
１６で反射される蛍光Ｘ線１７の波長帯域を変え、その
反射された蛍光Ｘ線１７を半導体検出器８に入射させ
る。具体的には、分析しようとする元素の蛍光Ｘ線のう
ち波長が最も短いものの臨界角よりも、視斜角φがわず
かに小さくなるように、全反射ミラー１６をその表面の
中心を通る紙面に垂直な軸Ｑを中心に回転させ、また、
半導体検出器８を軸Ｑを中心に円１２に沿って回転さ
せ、視斜角φと同じ角度の反射角φで反射される蛍光Ｘ
線１７の光路に位置させる。回動手段１０において、例
えば、前記軸Ｑに取り付けたポテンショメータ等によ
り、全反射ミラー１６および半導体検出器８が回転した
結果形成される入射角φ、反射角φが確認される。The rotating means 18 changes the wavelength band of the fluorescent X-rays 17 reflected by the total reflection mirror 16 and makes the reflected fluorescent X-rays 17 enter the semiconductor detector 8. Specifically, the total reflection mirror 16 is placed on a paper surface passing through the center of its surface so that the viewing angle φ is slightly smaller than the critical angle of the fluorescent X-ray of the element to be analyzed having the shortest wavelength. Around an axis Q perpendicular to
The semiconductor detector 8 is rotated along the circle 12 about the axis Q, and the fluorescence X reflected at the reflection angle φ of the same angle as the viewing angle φ
It is located in the optical path of line 17. In the rotating means 10, for example, the incident angle φ and the reflection angle φ formed by rotating the total reflection mirror 16 and the semiconductor detector 8 are confirmed by a potentiometer or the like attached to the axis Q.
【００２３】なお、このような視斜角φに設定した全反
射ミラー１６で反射される蛍光Ｘ線１７には、所望の波
長帯域の蛍光Ｘ線がすべて含まれるから、回動手段１８
は、第１実施形態の連動手段１０（図１）のように分光
素子６を回転させながら半導体検出器８も回転させて走
査させる必要はない。また、回動手段１８は、全反射ミ
ラー１６と半導体検出器８を歯車機構等の駆動機構によ
り機械的に連結し、その歯車機構等を単一のモータ等の
駆動源で駆動するものでもよいし、全反射ミラー１６と
半導体検出器８をそれぞれ独立した駆動源および駆動機
構で駆動し、それらの駆動源を適切に制御して前記のよ
うな動作を実現するものでもよい。The fluorescent X-rays 17 reflected by the total reflection mirror 16 set at such a viewing angle φ include all the fluorescent X-rays in a desired wavelength band.
It is not necessary to rotate and scan the semiconductor detector 8 while rotating the spectroscopic element 6 as in the interlocking means 10 (FIG. 1) of the first embodiment. Further, the rotating means 18 may be a means for mechanically connecting the total reflection mirror 16 and the semiconductor detector 8 by a driving mechanism such as a gear mechanism, and driving the gear mechanism or the like by a driving source such as a single motor. Then, the total reflection mirror 16 and the semiconductor detector 8 may be driven by independent drive sources and drive mechanisms, and the drive sources may be appropriately controlled to realize the above-described operation.
【００２４】次に、この装置の動作について説明する。
まず、例えばＡl 程度に軽い元素について分析する場合
には、分析しようとする元素の蛍光Ｘ線のうち波長が最
も短いものの臨界角よりも、視斜角φがわずかに小さく
なるように、回動手段１６により、全反射ミラー１６が
回動され、また、反射角φで反射される蛍光Ｘ線１７の
光路に位置するように、半導体検出器８が回動される。
そして、試料台２に載置された試料１にＸ線源４から１
次Ｘ線３が照射されると、試料１から発生した蛍光Ｘ線
５がソーラスリット１１を通過し、全反射ミラー１６で
一部が反射され、反射された蛍光Ｘ線１７の強度が半導
体検出器８で測定される。ここで、上述したような視斜
角φの設定により、分析しようとする元素のうち最も重
いものまたはそれよりも軽い元素の蛍光Ｘ線１７のみが
全反射ミラー１６で反射され、そのうち所望の元素の蛍
光Ｘ線が、エネルギー分解能の高い半導体検出器８およ
び図示しない波高分析器で電気的に分離され検出され
る。Next, the operation of this device will be described.
First, when analyzing an element as light as Al, for example, the rotation angle is set so that the viewing angle φ is slightly smaller than the critical angle of the fluorescent X-ray of the element to be analyzed having the shortest wavelength. By means 16, the total reflection mirror 16 is rotated, and the semiconductor detector 8 is rotated so as to be located in the optical path of the fluorescent X-ray 17 reflected at the reflection angle φ.
Then, the sample 1 placed on the sample stage 2
When the next X-ray 3 is irradiated, the fluorescent X-rays 5 generated from the sample 1 pass through the solar slit 11, are partially reflected by the total reflection mirror 16, and the intensity of the reflected fluorescent X-rays 17 is detected by a semiconductor. It is measured by the measuring device 8. Here, by setting the viewing angle φ as described above, only the fluorescent X-rays 17 of the heaviest or lighter element among the elements to be analyzed are reflected by the total reflection mirror 16, and the desired element Are electrically separated and detected by the semiconductor detector 8 having a high energy resolution and a wave height analyzer (not shown).
【００２５】また、例えばＭo 程度以上に重い元素につ
いて分析する場合にも、同様に、分析しようとする元素
の蛍光Ｘ線のうち波長が最も短いものの臨界角よりも、
視斜角φがわずかに小さくなるように設定され、分析し
ようとする元素のうち最も重いものまたはそれよりも軽
い元素の蛍光Ｘ線１７が全反射ミラー１６で反射され、
そのうち所望の元素の蛍光Ｘ線が、エネルギー分解能の
高い半導体検出器８および図示しない波高分析器で電気
的に分離され検出される。なお、この場合には、全反射
ミラー１６で反射される蛍光Ｘ線１７の波長帯域は広く
なり全反射ミラー１６による分光の効果は少なくなる
が、Ｍo 程度以上に重い元素の分析については、半導体
検出器８および波高分析器による電気的なエネルギー分
解のみで十分である。Also, for example, when analyzing an element heavy as much as Mo or more, similarly, the critical angle of the fluorescent X-ray of the element to be analyzed having the shortest wavelength is determined by the critical angle.
The viewing angle φ is set to be slightly smaller, and the fluorescent X-rays 17 of the heaviest or lighter element among the elements to be analyzed are reflected by the total reflection mirror 16,
Among them, fluorescent X-rays of a desired element are electrically separated and detected by the semiconductor detector 8 having high energy resolution and a wave height analyzer (not shown). In this case, the wavelength band of the fluorescent X-rays 17 reflected by the total reflection mirror 16 is widened and the effect of the spectral reflection by the total reflection mirror 16 is reduced. Only electrical energy decomposition by the detector 8 and the pulse height analyzer is sufficient.
【００２６】また、反射する蛍光Ｘ線１７の波長帯域を
変えるための全反射ミラー１６の回転は、前記第１実施
形態の装置において分光する蛍光Ｘ線７の波長を変える
ための分光素子６の回転に比較すると（図１）、はるか
に微小ですむので、半導体検出器８の入射口の幅が十分
大きければ、半導体検出器８は固定したままでも反射さ
れた蛍光Ｘ線１７を入射させることができる。このよう
な場合には、回動手段１８は、全反射ミラー１６のみを
回動させればよく、半導体検出器８を回動させる必要は
ない。The rotation of the total reflection mirror 16 for changing the wavelength band of the reflected fluorescent X-rays 17 is performed by changing the wavelength of the fluorescent X-rays 7 to be changed in the apparatus of the first embodiment. Compared to the rotation (FIG. 1), it is much smaller, so if the width of the entrance of the semiconductor detector 8 is sufficiently large, the reflected fluorescent X-rays 17 can be incident even if the semiconductor detector 8 is fixed. Can be. In such a case, the rotation means 18 need only rotate the total reflection mirror 16 and does not need to rotate the semiconductor detector 8.
【００２７】このように、第２実施形態の装置によれ
ば、まず、検出器として半導体検出器８のみを用いるの
で構成が簡単である。また、かかる回動手段１８により
広い波長範囲の蛍光Ｘ線５に対応しつつ、Ａl やＦe 程
度に軽い元素の分析では、全反射ミラー１６で所望の波
長帯域の蛍光Ｘ線１７のみを反射させるので分解能に優
れ、Ｍo 程度以上に重い元素の分析では、半導体検出器
８を用いているのでやはり分解能に優れる。さらに、分
光素子に比べはるかに反射効率の高い全反射ミラー１６
を用いるので、装置としてもＳ／Ｎ比が高い。したがっ
て、精度や感度が高く十分正確な分析ができる。As described above, according to the device of the second embodiment, first, only the semiconductor detector 8 is used as the detector, so that the configuration is simple. Moreover, while analyzing the X-rays 5 in a wide wavelength range by the rotating means 18 and analyzing the elements as light as Al and Fe, the total reflection mirror 16 reflects only the X-rays 17 in a desired wavelength band. Therefore, in the analysis of elements heavier than Mo or so, the semiconductor detector 8 is used, so that the resolution is also excellent. Further, the total reflection mirror 16 having a much higher reflection efficiency than the spectral element
Is used, the S / N ratio is also high for the device. Therefore, highly accurate and sensitive analysis can be performed with sufficient accuracy.
【００２８】なお、以上の第１、第２実施形態の装置で
は、ソーラスリット１１と平板の分光素子６または全反
射ミラー１６を組み合わせた平行光学系を用いたが、ピ
ンホールまたは線状孔のスリットと湾曲した分光素子ま
たは全反射ミラーを組み合わせた集中光学系を用いても
よい。集中光学系を用いる場合であって、いわゆるロー
ランド円を移動させない場合には、連動手段や回動手段
は、スリットも連動、回動させる必要がある。In the apparatus of the first and second embodiments, a parallel optical system in which the solar slit 11 and the flat spectral element 6 or the total reflection mirror 16 are combined is used. A concentrated optical system combining a slit and a curved spectral element or a total reflection mirror may be used. When a concentrated optical system is used and the so-called Rowland circle is not moved, the interlocking means and the rotating means need to interlock and rotate the slit.
【００２９】[0029]
【発明の効果】以上詳細に説明したように、本発明によ
れば、検出器として半導体検出器のみを用いた簡単な構
成で、精度や感度が高く十分正確な分析ができる。ま
た、ガスフロー型比例計数管を用いた装置のように、Ｐ
Ｒガス中のメタンガスが計数管の芯線に焼き付いて分解
能が低下することもないので、メンテナンスが楽で、長
期に安定して正確な分析ができる。As described in detail above, according to the present invention, a highly accurate and highly sensitive analysis can be performed with high accuracy and sensitivity with a simple configuration using only a semiconductor detector as a detector. In addition, as in an apparatus using a gas flow type proportional counter, P
Since the methane gas in the R gas does not stick to the core wire of the counter tube and the resolution does not decrease, maintenance is easy and stable and accurate analysis can be performed for a long time.
【図１】本発明の第１実施形態の蛍光Ｘ線分析装置を示
す概略図である。FIG. 1 is a schematic diagram showing a fluorescent X-ray analyzer according to a first embodiment of the present invention.
【図２】試料の微小部位を分析する場合等の同装置を示
す概略図である。FIG. 2 is a schematic diagram showing the same apparatus when analyzing a minute part of a sample.
【図３】本発明の第２実施形態の蛍光Ｘ線分析装置を示
す概略図である。FIG. 3 is a schematic diagram showing a fluorescent X-ray analyzer according to a second embodiment of the present invention.
１…試料、２…試料台、３…１次Ｘ線、４…Ｘ線源、５
…試料から発生した蛍光Ｘ線、６…分光素子、７…分光
素子で分光された蛍光Ｘ線、８…半導体検出器、１０…
連動手段、１１…スリット、１３…スリットを通過した
蛍光Ｘ線、１４…分光素子交換器、１５…移動手段、１
６…全反射ミラー、１７…全反射ミラーで反射された蛍
光Ｘ線、１８…回動手段。DESCRIPTION OF SYMBOLS 1 ... sample, 2 ... sample stage, 3 ... primary X-ray, 4 ... X-ray source, 5
... X-ray fluorescence emitted from the sample, 6 ... Spectroscopy element, 7 ... X-ray fluorescence separated by the spectroscopy element, 8 ... Semiconductor detector, 10 ...
Interlocking means, 11: slit, 13: fluorescent X-rays passing through the slit, 14: spectral element exchanger, 15: moving means, 1
6: total reflection mirror; 17: fluorescent X-ray reflected by the total reflection mirror; 18: rotating means.
Claims (3)
Ｘ線の光路に選択的に進出させて入射した蛍光Ｘ線を分
光させる分光素子交換器と、 前記分光素子で分光された蛍光Ｘ線の強度を測定する半
導体検出器と、 前記分光素子で分光される蛍光Ｘ線の波長を変えなが
ら、その分光された蛍光Ｘ線が前記半導体検出器に入射
するように、前記スリット、分光素子交換器および半導
体検出器のうち少なくとも分光素子交換器および半導体
検出器を連動させる連動手段とを備えた蛍光Ｘ線分析装
置。A sample stage on which a sample is placed; an X-ray source for irradiating the sample with primary X-rays; a slit for passing fluorescent X-rays generated from the sample; A spectroscopic element exchanger that selectively advances into the optical path of the fluorescent X-rays passing through the slit and disperses the incident fluorescent X-rays; and a semiconductor detector that measures the intensity of the fluorescent X-rays separated by the spectroscopic element. While changing the wavelength of the fluorescent X-rays split by the spectroscopic element, at least one of the slit, the spectral element exchanger, and the semiconductor detector so that the split fluorescent X-rays enter the semiconductor detector. An X-ray fluorescence analyzer comprising: an interlock for interlocking an element exchanger and a semiconductor detector.
を前記スリットおよび分光素子を介さずに測定する位置
に移動させる移動手段を備えた蛍光Ｘ線分析装置。2. The X-ray fluorescence analyzer according to claim 1, further comprising a moving unit that moves the semiconductor detector to a position where the intensity of the X-ray fluorescence generated from the sample is measured without passing through the slit and the spectral element. apparatus.
射ミラーと、 その全反射ミラーで反射された蛍光Ｘ線の強度を測定す
る半導体検出器と、 前記全反射ミラーで反射される蛍光Ｘ線の波長帯域を変
え、その反射された蛍光Ｘ線が前記半導体検出器に入射
するように、前記スリット、全反射ミラーおよび半導体
検出器のうち少なくとも全反射ミラーを回動させる回動
手段とを備えた蛍光Ｘ線分析装置。3. A sample stage on which a sample is placed, an X-ray source for irradiating the sample with primary X-rays, a slit for passing fluorescent X-rays generated from the sample, and a fluorescent X-ray passing through the slit A total reflection mirror that reflects a part of the light, a semiconductor detector that measures the intensity of the fluorescent X-ray reflected by the total reflection mirror, and a wavelength band of the fluorescent X-ray that is reflected by the total reflection mirror, An X-ray fluorescence analyzer, comprising: a rotating means for rotating at least the total reflection mirror of the slit, the total reflection mirror, and the semiconductor detector so that the reflected X-rays are incident on the semiconductor detector.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11142743A JP2000329714A (en) | 1999-05-24 | 1999-05-24 | X-ray fluorescence analyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11142743A JP2000329714A (en) | 1999-05-24 | 1999-05-24 | X-ray fluorescence analyzer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000329714A true JP2000329714A (en) | 2000-11-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11142743A Pending JP2000329714A (en) | 1999-05-24 | 1999-05-24 | X-ray fluorescence analyzer |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007017350A (en) * | 2005-07-08 | 2007-01-25 | Shimadzu Corp | X-ray analyzer |
| JP2007139754A (en) * | 2005-10-19 | 2007-06-07 | Rigaku Industrial Co | Fluorescence x-ray spectrometer, and program used therefor |
| JP2008256698A (en) * | 2007-04-05 | 2008-10-23 | Panalytical Bv | Fluorescent x-ray analyzer |
| JP2012058148A (en) * | 2010-09-10 | 2012-03-22 | Jeol Ltd | X-ray detection system |
| JP2012220337A (en) * | 2011-04-08 | 2012-11-12 | Hitachi Ltd | Analyzer for charged particle beam and analytical method therefor |
| EP2685247A1 (en) * | 2011-05-20 | 2014-01-15 | Rigaku Corporation | Wavelength-dispersive x-ray fluorescence analysis device |
| WO2018101133A1 (en) | 2016-12-01 | 2018-06-07 | 株式会社リガク | X-ray fluorescence analyzer |
| JPWO2021152928A1 (en) * | 2020-01-27 | 2021-08-05 |
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1999
- 1999-05-24 JP JP11142743A patent/JP2000329714A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007017350A (en) * | 2005-07-08 | 2007-01-25 | Shimadzu Corp | X-ray analyzer |
| JP4715345B2 (en) * | 2005-07-08 | 2011-07-06 | 株式会社島津製作所 | X-ray analyzer |
| JP2007139754A (en) * | 2005-10-19 | 2007-06-07 | Rigaku Industrial Co | Fluorescence x-ray spectrometer, and program used therefor |
| JP2008256698A (en) * | 2007-04-05 | 2008-10-23 | Panalytical Bv | Fluorescent x-ray analyzer |
| JP2012058148A (en) * | 2010-09-10 | 2012-03-22 | Jeol Ltd | X-ray detection system |
| JP2012220337A (en) * | 2011-04-08 | 2012-11-12 | Hitachi Ltd | Analyzer for charged particle beam and analytical method therefor |
| EP2685247A1 (en) * | 2011-05-20 | 2014-01-15 | Rigaku Corporation | Wavelength-dispersive x-ray fluorescence analysis device |
| EP2685247A4 (en) * | 2011-05-20 | 2014-10-08 | Rigaku Denki Co Ltd | Wavelength-dispersive x-ray fluorescence analysis device |
| WO2018101133A1 (en) | 2016-12-01 | 2018-06-07 | 株式会社リガク | X-ray fluorescence analyzer |
| JPWO2018101133A1 (en) * | 2016-12-01 | 2018-11-29 | 株式会社リガク | X-ray fluorescence analyzer |
| CN110088603A (en) * | 2016-12-01 | 2019-08-02 | 株式会社理学 | Fluorescent x-ray analyzer |
| US10514346B2 (en) | 2016-12-01 | 2019-12-24 | Rigaku Corporation | X-ray fluorescence spectrometer |
| JPWO2021152928A1 (en) * | 2020-01-27 | 2021-08-05 | ||
| JP7287507B2 (en) | 2020-01-27 | 2023-06-06 | 株式会社島津製作所 | X-ray fluorescence analyzer |
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